CN111521712B - Liquid chromatography analysis method for simultaneously determining contents of 3 sulfonamides and 4 quinolones - Google Patents
Liquid chromatography analysis method for simultaneously determining contents of 3 sulfonamides and 4 quinolones Download PDFInfo
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Abstract
The invention provides a high performance liquid chromatography analysis method for simultaneously determining the content of 3 sulfonamides and 4 quinolones antibiotics, belonging to the technical field of analysis. The method uses octadecylsilane chemically bonded silica as a filling agent, uses 0.3% sodium acetate solution-acetonitrile as a mobile phase for elution, can realize perfect separation and quantitative analysis of 3 kinds of sulfonamides and 4 kinds of quinolone antibiotics within 50min, has the advantages of strong specificity, high precision, good stability, high accuracy, simple and convenient operation, cheap and easily-obtained reagents and consumables, is suitable for quality control and analysis of a plurality of antibiotics in products in the pharmaceutical and food industries, and can effectively save the detection cost and time.
Description
Technical Field
The invention relates to the technical field of analysis, in particular to a liquid chromatography analysis method for simultaneously determining the contents of 3 sulfonamides and 4 quinolones.
Background
With the rapid development of economy, the living standard of people is continuously improved, and the wide use and the large amount of abuse of medicines lead to more and more serious residues of various medicines, so that the medicines are more and more valued by people.
However, most of the existing content determination methods in the current detection methods mainly determine the content of a single drug, and when the content of various different types of compounds is determined, the content needs to be detected respectively, so that the defects of complex operation, time consumption, labor consumption and the like exist.
The method also comprises a method for simultaneously determining the content of a plurality of sulfanilamide antibiotics or quinolone antibiotics, for example, a method for simultaneously determining 16 sulfanilamide drugs in beeswax by adopting a high performance liquid chromatography-tandem mass spectrometry is disclosed in a patent with the publication number of CN104931610B, specifically, a 1260 ultra-high performance liquid chromatography and 6460 triple quadrupole tandem mass spectrometry are adopted to detect the 16 sulfanilamide drugs, the result is that the 16 sulfanilamide drugs have a better linear relation in the range of 2ng/mL-50ng/mL, and the recovery rate of the 16 sulfanilamide drugs in a sample is 65% -127%, and the method is quick, sensitive and accurate, and can be used for qualitative and quantitative analysis of the residue of the 16 sulfanilamide drugs. However, the method needs to combine ultra-high performance liquid chromatography with a triple quadrupole tandem mass spectrometer, has the defects of complex operation and high detection cost, and has the problem that various different types of antibiotics cannot be detected simultaneously.
Disclosure of Invention
In view of the above, the present invention aims to provide a liquid chromatography method capable of simultaneously measuring the contents of 3 sulfonamides and 4 quinolones, which is simple in operation and low in cost.
Through research, the invention provides the following technical scheme:
the liquid chromatographic analysis method for simultaneously determining the contents of 3 sulfonamides and 4 quinolones comprises the following steps:
1) chromatographic conditions
Chromatographic column packing agent: octadecylsilane chemically bonded silica;
mobile phase: taking a mixed solution of an inorganic phase and an organic phase as a mobile phase;
flow rate: the flow rate is 1.0mL/min at 0-15 min;
the flow rate is 0.9mL/min at 15-31 min;
the flow rate is 1.0mL/min at 31-50 min;
and (3) an elution mode: isocratic elution;
detection wavelength: the detection wavelength of 0-15 min is 260 nm;
the detection wavelength is 270nm within 15-31 min;
the detection wavelength is 280nm within 31-50 min;
column temperature: 25-40 ℃;
2) preparation of test solution
Taking a test sample, and adding a mobile phase for dissolving to prepare a test sample solution;
3) single component control solutions and preparation of control solutions
Dissolving 3 sulfanilamide reference substances and 4 quinolone antibiotic reference substances respectively with mobile phase, filtering to remove impurities, and making into single-component reference substance solution and mixed reference substance solution;
4) determination of control solutions
Respectively injecting the single-component reference substance solution and the mixed reference substance solution into a liquid chromatograph, measuring under the condition that the detection wavelength is 260-280 nm, and recording a chromatogram;
5) measurement of test solution
Injecting the test solution into a liquid chromatograph, measuring by the same method, recording a chromatogram, and calculating the content of each antibiotic in the test solution by peak area according to an external standard method.
Preferably, the inorganic phase is a sodium acetate solution with the mass percentage of 0.3%.
Preferably, the organic phase is methanol, acetonitrile, n-butanol, n-propanol or isopropanol.
Preferably, the organic phase is acetonitrile.
Preferably, the pH value of the mobile phase is adjusted to 4.6 by using acetic acid solution.
Preferably, the volume ratio of the inorganic phase to the organic phase is 85: 15.
Preferably, the column temperature is 35 ℃.
Preferably, the 3 sulfonamides and 4 quinolones are sodium sulfathiazole, ciprofloxacin lactate, sodium sulfamethoxazole, pefloxacin mesylate, sodium sulfamonomethoxine, enrofloxacin and sarafloxacin hydrochloride respectively.
Preferably, the one-component control solution is prepared by the following method: precisely weighing sodium sulfathiazole, ciprofloxacin lactate, sodium sulfamethoxazole, pefloxacin mesylate and sulfamonomethoxineDissolving sodium, enrofloxacin and sarafloxacin hydrochloride in mobile phase, filtering to remove impurities, and preparing into solution with concentration of 0.2 mg/mL with the mobile phase-10.1 mg/mL of sulfathiazole sodium-1Ciprofloxacin lactate, 0.1 mg/mL-1Sulfamethol sodium, 0.1 mg/mL-1Pefloxacin mesylate, 0.1 mg. mL-1Sulfamonomethoxine sodium, 0.1 mg/mL-1Enrofloxacin and 0.2 mg/mL-1Sarafloxacin hydrochloride as a one-component control solution.
Preferably, the preparation of the mixed reference solution adopts the following method: precisely weighing the sulfathiazole sodium, the ciprofloxacin lactate, the sulfamethoxazole sodium, the pefloxacin mesylate, the sulfamonomethoxine sodium, the enrofloxacin and the sarafloxacin hydrochloride, dissolving by using a mobile phase, filtering impurities, and preparing a mixed reference substance solution with the concentration of 1mg/mL by using a mobile phase solution.
The invention has the beneficial effects that:
1) the high performance liquid chromatography analysis method for simultaneously determining the contents of 3 sulfonamides and 4 quinolone antibiotics provided by the invention uses cheap and easily-obtained octadecylsilane chemically bonded silica as a filler and uses 0.3% sodium acetate solution-acetonitrile as a mobile phase for elution, so that the complete separation and quantitative analysis of the 3 sulfonamides and 4 quinolone antibiotics can be realized within 50 min;
2) the high performance liquid chromatography analysis method for simultaneously determining the content of the quinolone antibiotics in the 3 sulfonamides and 4 has the advantages of strong specificity, high precision, good stability, high accuracy, simple and convenient operation, cheap and easily-obtained reagents and consumables, suitability for quality control and analysis of various antibiotics in products in the pharmaceutical and food industries, and effective saving of detection cost and time.
Drawings
FIG. 1 is a chromatogram of a mixed control solution.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The liquid chromatography analysis method for simultaneously determining the contents of 3 sulfonamides and 4 quinolones in the embodiment comprises the following steps:
1) chromatographic conditions
Chromatographic column packing agent: octadecylsilane bonded silica (C18250 mm X4.6, 5 μm);
mobile phase: in a volume ratio of 85:15, taking a mixed solution of 0.3 percent sodium acetate and acetonitrile as a mobile phase, and adjusting the pH value to 4.6 by using an acetic acid solution;
flow rate: the flow rate is 1.0mL/min at 0-15 min;
the flow rate is 0.9mL/min at 15-31 min;
the flow rate is 1.0mL/min at 31-50 min;
and (3) an elution mode: isocratic elution;
detection wavelength: the detection wavelength of 0-15 min is 260 nm;
the detection wavelength is 270nm within 15-31 min;
the detection wavelength is 280nm within 31-50 min;
sample introduction amount: 20 mu L of the solution;
column temperature: 35 ℃;
2) preparation of test solution
Precisely weighing 10.02mg of sulfathiazole sodium, 4.86mg of ciprofloxacin lactate, 5.72mg of sulfamethoxazole sodium, 4.84mg of pefloxacin mesylate, 4.93mg of sulfamonomethoxine sodium, 4.96mg of enrofloxacin and 11.28mg of sarafloxacin hydrochloride, and putting the components in a 50ml volumetric flask in a volume ratio of 85: dissolving the mixed solution of 15 percent of sodium acetate and acetonitrile to prepare a mixed test solution;
3) preparation of Single component control solutions and Mixed control solutions
Precisely weighing standard reference substances of sodium sulfathiazole, ciprofloxacin lactate, sodium sulfamethoxazole, pefloxacin mesylate, sodium sulfamonomethoxine, enrofloxacin and sarafloxacin hydrochloridePlacing the mixture into a volumetric flask, and adding a solvent with the volume ratio of 85:15, 0.3% sodium acetate and acetonitrile, to a concentration of 0.2 mg/mL-10.1 mg/mL of sulfathiazole sodium-1Ciprofloxacin lactate, 0.1 mg/mL-1Sulfamethol sodium, 0.1 mg/mL-1Pefloxacin mesylate, 0.1 mg. mL-1Sulfamonomethoxine sodium, 0.1 mg/mL-1Enrofloxacin and 0.2 mg/mL-1Sarafloxacin hydrochloride as a single-component control solution;
precisely weighing standard reference substances of sulfathiazole sodium, ciprofloxacin lactate, sulfamethoxazole sodium, pefloxacin mesylate, sulfamonomethoxine sodium, enrofloxacin and sarafloxacin hydrochloride, mixing and placing the standard reference substances in a volumetric flask in a volume ratio of 85:15, dissolving the mixture of 0.3 percent sodium acetate and acetonitrile, filtering impurities, and then adding a solvent with the volume ratio of 85:15, preparing a mixed reference substance solution with the concentration of 1mg/mL by using a 0.3% sodium acetate and acetonitrile mixed solution;
4) determination of control solutions
Respectively injecting 20 μ L of the single-component reference substance solution and the mixed reference substance solution into a liquid chromatograph, and recording chromatogram;
5) measurement of test solution
Injecting 20 μ L of the mixed sample solution into a liquid chromatograph, recording chromatogram, measuring under the same chromatographic condition, and calculating the content of the drug in the mixed sample solution by peak area according to an external standard method.
Determining the peak positions of the 7 antibiotics by analyzing the chromatogram of the single component control solution, and then comparing and analyzing the chromatogram of the mixed control solution and the chromatogram of the single component control solution, thereby determining the substances corresponding to each characteristic peak in the chromatogram of the mixed control solution.
The substance corresponding to each characteristic peak in the chromatogram of the control solution is shown in FIG. 1. As can be seen from the analysis in FIG. 1, 3 kinds of sulfonamides and 4 kinds of quinolone antibiotics can be completely separated and quantitatively analyzed within 50 min.
Verification of content determination method
1. Specificity
Respectively and precisely measuring 20 μ L of each of the mixed reference solution and the negative test solution containing 7 antibiotic components, injecting into a liquid chromatograph, and recording chromatogram. By comparing the chromatograms of each negative test solution of the mixed control solution and 7 antibiotic components, the average retention time of the chromatographic peaks of the 7 antibiotic components is shown in table 1.
TABLE 1 average retention time of chromatographic peak for each component
The chromatogram of each negative test sample solution of the mixed reference solution and the 7 antibiotics proves that the retention time of each component is consistent, the negative test samples of each component at the retention time position are not obviously interfered, and further proves that under the chromatographic condition of the invention, each component is well retained and can be perfectly separated.
2. Linear correlation
Accurately weighing 12.26mg of sulfathiazole sodium, 12.55mg of ciprofloxacin lactate, 12.33mg of sulfamethoxazole sodium, 12.04mg of pefloxacin mesylate, 11.77mg of sulfamonomethoxine sodium, 11.57mg of enrofloxacin and 11.40mg of sarafloxacin hydrochloride, putting into a 100ml volumetric flask, and adding the components in a volume ratio of 85:15, and dissolving the mixture of 0.3 percent sodium acetate and acetonitrile to prepare a reference solution. Respectively and precisely sucking a proper amount of reference substance solution, wherein the volume ratio of the reference substance solution to the reference substance solution is 85:15, 0.3% sodium acetate and acetonitrile, respectively, to 250.00, 125.00, 50.00, 25.00, 12.50, 5.00, 1.25. mu.g/mL-1The different reference substance solutions are measured according to the chromatographic conditions under the content measurement items, a standard curve is plotted and drawn by taking the concentration X as a horizontal coordinate and the peak area y as a vertical coordinate, and the linear regression equation and the correlation coefficient R of the 3 sulfonamides and 4 quinolone antibiotics are obtained and are shown in the table 2.
TABLE 2 results of the linear relationship of the components
From the analysis in table 2, it can be seen that 7 different antibiotics are all in a linear range, and the correlation coefficient R is all above 0.99, which proves that the peak area and the concentration present a good linear relationship.
3. Accuracy of
Sample recovery rate test: precisely measuring 9 parts of test solution with known antibiotic content, wherein each 3 parts is 1 group, adding 1mL, 3mL and 5mL of mixed control solution into each group according to low, medium and high concentrations, shaking up, diluting to a scale mark, precisely measuring 20 μ L, injecting into a liquid chromatograph, recording chromatogram, and calculating average sample addition recovery rate and Relative Standard Deviation (RSD) of 7 antibiotic components, wherein the results are shown in Table 3.
TABLE 3 results of accuracy measurements
| Composition (I) | Average sample recovery (%) | RSD(％) |
| Sulfathiazole sodium salt | 99.34 | 1.12 |
| Lactic acid ciprofloxacin | 98.92 | 1.51 |
| Sulfamethol sodium | 100.24 | 1.07 |
| Pefloxacin mesylate | 100.08 | 1.09 |
| Sulfamonomethoxine sodium | 99.89 | 1.48 |
| Enrofloxacin | 98.91 | 1.74 |
| Sarafloxacin hydrochloride | 97.83 | 1.89 |
From the analysis in table 3, the average sample recovery rate of 7 antibiotic components is greater than 97%, and the RSD is less than 1.9%, thus demonstrating the high accuracy of the present invention.
4. Stability of
Preparing a mixed reference solution, precisely measuring 20 mu L of the mixed reference solution for 0, 4, 8 and 12 hours respectively, injecting into a liquid chromatograph, recording a chromatogram, injecting 3 times at each time point, and calculating a Relative Standard Deviation (RSD) value according to the peak area measured for 4 times of each antibiotic chromatographic peak, wherein the result is shown in Table 4.
Table 4 stability test results
| Composition (I) | RSD(％) |
| Sulfathiazole sodium salt | 1.62 |
| Lactic acid ciprofloxacin | 1.83 |
| Sulfamethol sodium | 1.94 |
| Pefloxacin mesylate | 2.19 |
| Sulfamonomethoxine sodium | 1.86 |
| Enrofloxacin | 1.67 |
| Sarafloxacin hydrochloride | 1.81 |
As can be seen from the analysis in Table 4, the peak areas RSD of the chromatographic peaks of the 7 antibiotics all meet the precision requirement, thereby proving that the method of the invention has good stability.
5. Precision degree
Precisely measuring 20 μ L of the mixed reference solution, injecting into a liquid chromatograph, recording chromatogram, and repeating for 6 times. Relative Standard Deviation (RSD) was calculated as the peak area of 6 measurements of each antibiotic chromatographic peak. The results are shown in Table 5.
TABLE 5 results of precision investigation
| Composition (I) | RSD(％) |
| Sulfathiazole sodium salt | 1.69 |
| Lactic acid ciprofloxacin | 1.93 |
| Sulfamethol sodium | 2.05 |
| Pefloxacin mesylate | 2.61 |
| Sulfamonomethoxine sodium | 1.89 |
| Enrofloxacin | 2.38 |
| Sarafloxacin hydrochloride | 2.05 |
As can be seen from the analysis in Table 5, the peak areas RSD of the chromatographic peaks of the antibiotic components in 7 all meet the precision requirement, thus proving that the method of the invention has good precision.
The above examples of the present invention are merely examples for illustrating the present invention, and are not intended to limit the embodiments of the present invention, and the scope of the present invention is not limited thereto. Variations and modifications in other variations will occur to those skilled in the art upon reading the foregoing description. Not all embodiments are exhaustive. All obvious changes and modifications of the present invention are within the scope of the present invention. The protection scope of the invention is subject to the claims.
Claims (4)
1. The liquid chromatography analysis method for simultaneously determining the contents of 3 sulfonamides and 4 quinolones is characterized by comprising the following steps of:
1) chromatographic conditions
Chromatographic column packing agent: octadecylsilane chemically bonded silica;
mobile phase: taking a mixed solution of an inorganic phase and an organic phase as a mobile phase; the volume ratio of the inorganic phase to the organic phase is 85: 15; the inorganic phase is a sodium acetate solution with the mass percentage of 0.3%; the organic phase is acetonitrile; adjusting the pH value of the mobile phase to 4.6 by adopting an acetic acid solution;
flow rate: the flow rate is 1.0mL/min at 0-15 min;
the flow rate is 0.9mL/min at 15-31 min;
the flow rate is 1.0mL/min at 31-50 min;
and (3) an elution mode: isocratic elution;
detection wavelength: the detection wavelength of 0-15 min is 260 nm;
the detection wavelength is 270nm within 15-31 min;
the detection wavelength is 280nm within 31-50 min;
column temperature: 25-40 ℃;
2) preparation of test solution
Dissolving a test sample in a mobile phase to prepare a test sample solution;
3) preparation of Single component control solutions and Mixed control solutions
Dissolving 3 sulfonamides and 4 quinolones with mobile phase, filtering to remove impurities, and making into single-component and mixed reference solutions; the 3 kinds of sulfonamides and the 4 kinds of quinolones are respectively sodium sulfathiazole, ciprofloxacin lactate, sodium sulfadimidine, pefloxacin mesylate, sodium sulfamonomethoxine, enrofloxacin and sarafloxacin hydrochloride;
4) determination of control solutions
Respectively injecting the single-component reference substance solution and the mixed reference substance solution into a liquid chromatograph, measuring under the condition that the detection wavelength is 260-280 nm, and recording a chromatogram;
5) measurement of test solution
Injecting the test solution into a liquid chromatograph, measuring by the same method, recording a chromatogram, and calculating the content of each antibiotic in the test solution by peak area according to an external standard method.
2. The method for simultaneously measuring the contents of 3 sulfonamides and 4 quinolones according to claim 1, wherein the column temperature is 35 ℃.
3. The method for simultaneously measuring the contents of 3 sulfonamides and 4 quinolones according to claim 1, wherein the monocomponent control solution is prepared by the following method: precisely weighing sodium sulfathiazole, ciprofloxacin lactate, sodium sulfamethoxazole, pefloxacin mesylate, sodium sulfamonomethoxine, enrofloxacin and sarafloxacin hydrochloride, dissolving with mobile phase, filtering to remove impurities, and preparing into solution with concentration of 0.2 mg/mL with mobile phase solution-10.1 mg/mL of sulfathiazole sodium-1Ciprofloxacin lactate, 0.1 mg/mL-1Sulfamethol sodium, 0.1 mg/mL-1Pefloxacin mesylate, 0.1 mg. mL-1Sulfamonomethoxine sodium, 0.1 mg/mL-1Enrofloxacin and 0.2 mg/mL-1Sarafloxacin hydrochloride as a one-component control solution.
4. The method for simultaneously determining the contents of 3 sulfonamides and 4 quinolones according to claim 1, wherein the mixed control solution is prepared by the following method: precisely weighing the sulfathiazole sodium, the ciprofloxacin lactate, the sulfamethoxazole sodium, the pefloxacin mesylate, the sulfamonomethoxine sodium, the enrofloxacin and the sarafloxacin hydrochloride, dissolving by using a mobile phase, filtering impurities, and preparing a mixed reference substance solution with the concentration of 1mg/mL by using a mobile phase solution.
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